HRID963698
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of (5-methoxy-1,2,3,4-tetrahydro-2-naphthyl)methanol (1.00 g) in dry pyridine (10 ml) was added p-toluenesulfonyl chloride (1.15 g) under ice bath cooling. The mixture was stirred for 1 day at room temperature and partitioned between ethyl acetate and water. The organic layer was separated, washed with water (twice), 1N hydrochloric acid and brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1) to give (5-methoxy-1,2,3,4-tetrahydro-2-naphthyl)methyl p-toluenesulfonate (1.70 g) as a white powder. mp: 81°-82° C.
WORKUP
后处理
- temperaturecooling
- custompartitioned between ethyl acetate and water
- customThe organic layer was separated
- washwashed with water (twice), 1N hydrochloric acid and brine
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1)